title: Application of high-speed counter-current chromatography for preparative separation of cyclic peptides from Vaccaria segetalis.
abstract: Following an initial clean-up step on silica gel, high-speed counter-current chromatography (HSCCC) was used to separate cyclic peptides from an extract of the seeds of Vaccaria segetalis. The two-phase solvent system used for HSCCC separation was composed of petroleum ether-ethyl acetate-methanol-water at an optimized volume ratio of 0.5:3.5:1:5. From 190 mg of crude extract, 38.0 mg of segetalin B and 28.5 mg of segetalin A were obtained with purities of 98.1% and 95.6% as determined by HPLC, respectively. The chemical structures of the target compounds were confirmed by high resolution electrospray ionization time of flight MS (HRESI-TOF-MS) and (1)H NMR analyses.
authors.affiliation: Institute of Chinese Material Medical, China Academy of Chinese Medical Sciences, Beijing, China.
authors.forename: Xiao
authors.initials: X
authors.lastname: Wang
authors.forename: Hongjing
authors.initials: H
authors.lastname: Dong
authors.forename: Yuqin
authors.initials: Y
authors.lastname: Liu
authors.forename: Bin
authors.initials: B
authors.lastname: Yang
authors.forename: Xia
authors.initials: X
authors.lastname: Wang
authors.forename: Luqi
authors.initials: L
authors.lastname: Huang
mesh_terms: D000085:Acetates / Q000737:chemistry; D000473:Alkanes / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid; D003377:Countercurrent Distribution / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D000432:Methanol / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular; D010456:Peptides, Cyclic / Q000302:isolation & purification*; D012639:Seeds / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization; D031245:Vaccaria / Q000737:chemistry*
chemical_list: D000085:Acetates; D000473:Alkanes; D004365:Drugs, Chinese Herbal; D010456:Peptides, Cyclic; C101980:segetalin A; C101981:segetalin B; C007650:ethyl acetate; C004544:naphtha; D000432:Methanol